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Because optics to reflect the body on the biological activity, the toxicity and metabolism mechanism differ from, therefore to reflects body's preparation great importance solely. But the chiral Alpha - benzene ethylamine is the preparation to reflects one of solely body's important intermediates, it both may make the racemic modification the chiral resolution reagent, and may make the chiral raw material which is asymmetrical synthesizes, therefore its preparation and the analysis have the important meaning. This article used the tartaric acid and the cinnamic acid has conducted the resolution research separately to it. this article first obtains from the racemization Alpha - benzene ethylamine's preparation, responded through Liu Carter, takes Alpha - the benzene ethylamine using the ammonium formiate and the hypnone mix add-on produce by heat. In the experiment the temperature control tests the successful or not key, must the control response temperature in 180℃-185℃. This experiment passes through is defeated many times, succeeded the system to take Alpha - the benzene ethylamine, the production rate is 41.9% finally. In the resolution experiment, I have selected the laboratory commonly used chemistry resolution law, the choice resolution medicinal preparation for the tartaric acid and the cinnamic acid, and has carried on the comparison to two kind of resolution medicinal preparation's resolution effect, after artificial factors, may determine, in the laboratory, prepares the few optical activity Alpha - benzene ethylamine using the cinnamic acid the experiment in the operation and the synthesis effect, is friends with one compared to the tartaric acid resolution law. In the tartaric acid resolution experiment the system results in S-(-)--The benzene ethylamine optical rotation for α25D=1.2, density d=0.0676g/ml, [Alpha] D25=17.75, the optical activity purity is 44.22%, in the cinnamic acid resolution experiment, R-α - the benzene ethylamine and S-α - the benzene ethylamine's optical activity purity respectively is 78.1% and 81.5%
Moreover in the experiment, I revised in the experiment book to test some unreasonable places about this, for example after the hypnone and the ammonium formiate responded, must use the laundering mixture, returned to the reaction bulb but actually the lower level organic matter, but the water level used the chloroform extract 2 times, then returned to the extracted liquid the reaction bulb to carry on but actually the distillation, however distilled in the actual operation is very actually difficult to carry on, because the chloroform boiling point was very low (61.7℃). If temperature control not, when easily evaporation the reactant, is quite difficult in the operation. Moreover the chloroform toxicity is quite big, therefore, selected the boiling point in here me to be relatively high moreover the toxic relatively low toluene to take the extracting agent (110.8℃). In the experiment reduced the operation difficulty.

Abstract

As the optical enantiomers in the biological activity, toxicity and mechanism of the metabolism is different, so a single enantiomer preparation of paramount importance. The chiral α-phenylethylamine is a complex preparation of single enantiomers, one of the important intermediate, which can be raceme chiral separation of the reagents, but also for the asymmetric synthesis of chiral materials, it Preparation and analysis of great significance. In this paper, the use of tartaric acid and cinnamic acid, respectively, were split on their research.

In this paper, first of all from racemic α-phenylethylamine start the preparation, through the reaction of Mr Carter, the use of ammonium perchlorate and a mixture of acetophenone check the heating system of α-phenylethylamine. Experiment temperature control is key to the success of the experiment, the reaction temperature must be controlled at 180 ℃ -185 ℃. After repeated failures in this experiment, the ultimate success of the preparation of the α-phenylethylamine, the yield was 41.9%. In the separation experiment, I chose the commonly used laboratory method of chemical separation, separation agent of choice for the tartaric acid and cinnamic acid, and the two agents split the effect of separation were compared, except for some man-made factors can be identified in the laboratory using a small amount of cinnamic acid to the preparation of optically active α-phenylethylamine in the operation of the experimental and synthetic results, the split method is better than some of tartaric acid. Tartaric acid obtained by resolution of the experiment the S-(-) -  - Optical Rotation for phenylethylamine α25D = 1.2, the density of d = 0.0676g/ml, [α] D25 = 17.75, Polarimetry purity 44.22%, cinnamic acid removed sub-experiments, R-α-phenylethylamine and S-α-phenylethylamine, respectively, for the optically active purity 78.1% and 81.5%

Also in the experiment, I modified the experimental book unreasonable on this experiment, such as acetophenone and in the Ammonium reaction after washing use a mixture of organic matter back to the lower reaction bottle, and the water layer is extraction with chloroform 2 times, and then extract the response back to distillation bottles, but in practice it is difficult to carry out distillation, low boiling point because of chloroform (61.7 ℃). If the temperature controlled easy to dry reactant, in the operation more difficult. Also compare the toxicity of chloroform, and, therefore, I chose a relatively high boiling point and relatively low toxicity of toluene as the extractant (110.8 ℃). In the experiment to reduce the difficulty of the operation.

Abstract

As the optical enantiomers in the biological activity, toxicity and mechanism of the metabolism is different, so a single enantiomer preparation of paramount importance. The chiral α-phenylethylamine is a complex preparation of single enantiomers, one of the important intermediate, which can be raceme chiral separation of the reagents, but also for the asymmetric synthesis of chiral materials, it Preparation and analysis of great significance. In this paper, the use of tartaric acid and cinnamic acid, respectively, were split on their research.

In this paper, first of all from racemic α-phenylethylamine start the preparation, through the reaction of Mr Carter, the use of ammonium perchlorate and a mixture of acetophenone check the heating system of α-phenylethylamine. Experiment temperature control is key to the success of the experiment, the reaction temperature must be controlled at 180 ℃ -185 ℃. After repeated failures in this experiment, the ultimate success of the preparation of the α-phenylethylamine, the yield was 41.9%. In the separation experiment, I chose the commonly used laboratory method of chemical separation, separation agent of choice for the tartaric acid and cinnamic acid, and the two agents split the effect of separation were compared, except for some man-made factors can be identified in the laboratory using a small amount of cinnamic acid to the preparation of optically active α-phenylethylamine in the operation of the experimental and synthetic results, the split method is better than some of tartaric acid. Tartaric acid obtained by resolution of the experiment the S-(-) -  - Optical Rotation for phenylethylamine α25D = 1.2, the density of d = 0.0676g/ml, [α] D25 = 17.75, Polarimetry purity 44.22%, cinnamic acid removed sub-experiments, R-α-phenylethylamine and S-α-phenylethylamine, respectively, for the optically active purity 78.1% and 81.5%

Also in the experiment, I modified the experimental book unreasonable on this experiment, such as acetophenone and in the Ammonium reaction after washing use a mixture of organic matter back to the lower reaction bottle, and the water layer is extraction with chloroform 2 times, and then extract the response back to distillation bottles, but in practice it is difficult to carry out distillation, low boiling point because of chloroform (61.7 ℃). If the temperature controlled easy to dry reactant, in the operation more difficult. Also compare the toxicity of chloroform, and, therefore, I chose a relatively high boiling point and relatively low toxicity of toluene as the extractant (110.8 ℃). In the experiment to reduce the difficulty of the operation.

Key word: α-Benzene ethylamine Chiral synthesis Chiral resolution

As the optical enantiomers in the biological activity, toxicity and mechanism of the metabolism is different, so a single enantiomer preparation of paramount importance. The chiral α-phenylethylamine is a complex preparation of single enantiomers, one of the important intermediate, which can be raceme chiral separation of the reagents, but also for the asymmetric synthesis of chiral materials, it Preparation and analysis of great significance. In this paper, the use of tartaric acid and cinnamic acid, respectively, were split on their research.
In this paper, first of all from racemic α-phenylethylamine start the preparation, through the reaction of Mr Carter, the use of ammonium perchlorate and a mixture of acetophenone check the heating system of α-phenylethylamine. Experiment temperature control is key to the success of the experiment, the reaction temperature must be controlled at 180 ℃ -185 ℃. After repeated failures in this experiment, the ultimate success of the preparation of the α-phenylethylamine, the yield was 41.9%. In the separation experiment, I chose the commonly used laboratory method of chemical separation, separation agent of choice for the tartaric acid and cinnamic acid, and the two agents split the effect of separation were compared, except for some man-made factors can be identified in the laboratory using a small amount of cinnamic acid to the preparation of optically active α-phenylethylamine in the operation of the experimental and synthetic results, the split method is better than some of tartaric acid. Tartaric acid obtained by resolution of the experiment the S-(-) -  - Optical Rotation for phenylethylamine α25D = 1.2, the density of d = 0.0676g/ml, [α] D25 = 17.75, Polarimetry purity 44.22%, cinnamic acid removed sub-experiments, R-α-phenylethylamine and S-α-phenylethylamine of the optical rotation for the purity of 78.1%, respectively, and 81.5%
Also in the experiment, I modified the experimental book unreasonable on this experiment, such as acetophenone and in the Ammonium reaction after washing use a mixture of organic matter back to the lower reaction bottle, and the water layer is extraction with chloroform 2 times, and then extract the response back to distillation bottles, but in practice it is difficult to carry out distillation, low boiling point because of chloroform (61.7 ℃). If the temperature controlled easy to dry reactant, in the operation more difficult. Also compare the toxicity of chloroform, and, therefore, I chose a relatively high boiling point and relatively low toxicity of toluene as the extractant (110.8 ℃). In the experiment to reduce the difficulty of the operation.

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